用UHPLC-MS/MS法测定比格犬血浆中拉西地平的浓度
Determination of lacidipine in Beagle dog plasma by UHPLC-MS/MS method
王燕燕 1姜宜宏 1赵小英 1周真宇 1李晓红 2阎成炟 3秦峰1
作者信息
- 1. 沈阳药科大学药学院,辽宁本溪 117000
- 2. 中国医科大学附属第一医院药学部,辽宁沈阳 110001
- 3. 中国医科大学附属第一医院药物临床试验Ⅰ期中心,辽宁沈阳 110001
- 折叠
摘要
目的 建立一种测定比格犬血浆中拉西地平的超高效液相色谱-串联质谱方法.方法 用蛋白沉淀法进行预处理,内标为尼莫地平.色谱柱:ACQUITY UPLC® BEH C8(2.1 mm × 50.0 mm,1.7 μm),流动相:100％水含5 mmol·L-1醋酸铵-100％乙腈,流速:0.7 mL·min-1,柱温:40℃,自动进样器温度:4℃,进样量:20 μL.用电喷雾离子化源,正离子模式,多反应监测.考察该方法的专属性、残留效应、标准曲线与定量下限、精密度与回收率、基质效应、稳定性.结果 拉西地平在0.10～50.0 ng·mL-1内线性关系良好,r=0.996 6,定量下限为0.10 ng·mL-1,专属性良好,批内和批间相对标准偏差不超过12％,提取回收率高于80％,稳定性结果良好.结论 本方法灵敏度高、操作简单、分析时间短,适用于比格犬血浆中拉西地平的药代动力学研究.
Abstract
Objective To establish an ultra high performance liquid chromatography-tandem mass spectrometry method for the determination of lacidipine in plasma of beagle dogs was established.Methods It was pretreated by protein precipitation method and the internal standard was nimodipine.Chromatographic column:ACQUITYUPLC® BEH C8(2.1 mm x50.0 mm,1.7 μm),mobile phase:100％water containing 5 mmol·L-1 ammonium acetate-100％acetonitrile,flow rate:0.7 mL·min-1,column temperature:40 ℃,automatic injector temperature:4 ℃,injection volume:20 μL.Electrospray ionization source,positive ion mode,multi-reaction monitoring.The specificity,residual effect,standard curve and quantitative lower limit,precision and recovery,matrix effect and stability of the method were investigated.Results Lacidipine has a good linear relationship in the range of 0.10-50.0 ng·mL-1,r=0.996 6,the lower limit of quantification was 0.10 ng·mL-1.The specificity was good.The intra-and inter-relative standard deviation was less than 12％.The extraction recovery was higher than 80％,and the stability was good.Conclusion The method has the advantages of high sensitivity,simple operation and short analysis time,and was suitable for the pharmacokinetic study of lacidipine in Beagle dog plasma.
关键词
拉西地平/超高效液相色谱-串联质谱法/血药浓度Key words
lacidipine/ultra-high performance liquid chromatography-tandem mass spectrometry/drug plasma concentration引用本文复制引用
基金项目
沈阳药科大学中青年教师事业发展支持计划基金资助项目(ZQN202305)
出版年
2024
国家科技期刊平台
NSTL
万方数据